Hitachi HF2000 TEM, Operation Manual

Page 1: ... sure you follow what I told you ask before you touch the TEM if you do not know the consequence of your action Takamichi MIYAZAKI June 2009 Contents 1 Startup 2 Set the sample loading 3 Applying High Voltage 4 Prepare for beam alignment 5 Correct condenser astigmatism 6 Z height adjustment 7 Voltage center 8 Image focus and Objective lens astigmatism correction 9 Selected area electron diffractio...

Page 2: ...e out position 0 c GV Gun Valve is Closed d ACC VOLTAGE off HV on at 200kV e Sample position X 0 Y 0 Sample tilts 0 f Bright Dark field selector set at Bright field g Microscope is at ANA1 mode h Magnification 1000K 1500K i Normally the sample holder stays TEM It is situated at position A j Lens Current C1 C2 OBJ not 0 k Unexposed film number 50 FULL Film number 1 0 After confirmation of the stand...

Page 3: ...sample holder into TEM Follow the route indicated in the diagram below to load your sample holder into the TEM 1 Insert the sample holder horizontally along and press it then turn the switch to EVAC 2 When electron sound rings turn the holder clockwise till it stops 3 Let the sample holder go into the TEM horizontally along and smoothly The sample holder must be under control 4 Turn the sample hol...

Page 4: ...up to 200kV Then V1 and V2 Voltage rises gradually up to the setting value watch the ACC VOLT on the CRT monitor Enter the V1 Voltage and IF current on the log book Yellow book When the emission current drops below 10µA press I1C and recalibrate extraction voltage to raise the emission current to 30µA The beam wander off during the process but return by the end of the I1C state Repeat alignment pr...

Page 5: ...el make the caustic as round or axial symmetry And using the 3rd order stigmator left sub panel makes the caustic as symmetry The 3rd order correction will be slight and the controls should be close to the center positions The correctly aligned caustic will appear as a circle with Star in TEM mode The image is shown below Insert condenser aperture First aperture and minimize the swinging beam usin...

Page 6: ...sing wobblers method or minimum contrast method for the image focus 7 Voltage center Move edge of sample Turn on HVM HV MODULATION right panel The image feature may oscillate Adjust BEAM TILT right sub panel to minimize the vibration of the feature Turn off HVM right panel Repeat the alignment procedure a few times because the beam tilt and objective stigmatism correction have disturbed the conden...

Page 7: ...and Y control knobs so that granularity a amorphous becomes finer granularity as shown in the figure below 9 Image focus and Objective lens astigmatism correction Including Selected area electron diffraction SAED This is to tell you how to correct objective lens astigmatism using amorphous film which is useful in recording a high resolution image Center a small hole particle the sharp edge of samp...

Page 8: ...SAED Note If the central spot is not at the viewing center center it using the INTER ALIGN X and Y knobs left sub panel If the spot is not round make it round using INTER STIG X and Y knobs left sub panel Insert the objective aperture into the beam by turning the aperture handle clockwise Press ZOOM to see a bright field image Adjust fine focus and OBJ STIG if necessary Adjust Brightness so that A...

Page 9: ...E control knob The set exposure time is displayed at the bottom right on the CRT Optimum exposure time lines for Bright field image 1 to 4 seconds Dark field image 12 to 30 seconds Selected area diffraction pattern 0 5 to 1 seconds Nano beam diffraction pattern 8 to 16 seconds Press the PHOTO key to start recording 12 CCD camera Turn on the power to TV monitor and control Open the beam by turning ...

Page 10: ...tism is not corrected rotating motion in a specific direction is observed Adjust the BTX and BTVX controls on the left sub panel so that non directional image rotation is observed as shown below Turn the WOBBLER ANGELE control counterclockwise by 3 steps When astigmatism is not corrected adjust the BTY and BTVY controls on the left sub panel so that non directional image rotation is observed as sh...

Page 11: ...t condenser aperture Second aperture and minimize the swinging beam using the condenser X Y adjustment screws when passing through crossover Sample tilt see Sec 9 SAED Change the condenser aperture to forth aperture And minimize the swinging beam using the condenser X Y adjustment screws when passing through crossover Adjust the objective focus and confirm to select an interesting area Press DIFF ...

Page 12: ...lly unload the sample holder and set the holder A position after removing sample 19 Film exchange Wear gloves Turn off all lights room light CRT monitor panel light CCD monitor except the safelight Turn the switch of the desiccators down to Air position After a few minutes open the desiccators door take out full film magazine and prepare empty receiver Open the cover of the camera chamber and turn...

Page 13: ...osed film and the light shielding plate 2 Place film in the magazine 3 After loading the films don t forget to insert the light shielding plate Open the desiccator s door and introduce the full film magazine Turn the knob to EVAC Reset film number to 50 on the CRT using the keypad Listen for the shielding plate to properly feed through into the film receiver Change the FILM NUMBER to 0 using the k...

Page 14: ... The objective aperture will generate hard x rays and burn out the detector 2 The EDS procedure Make sure to turn off the column pressure gauge and insert condenser aperture 2nd aperture Turn on the power switch of the EDS workstation Screen Click Spectral Display icon Select Acquire Parameter Set up Set the max energy to 20 48 keV Find region of interest and focus it properly with brightness knob...

Page 15: ...m for average atomic number absorption and fluorescence factors which influence spectrum differences between elements in pure and composition Used in metallurgical SEM applications Proza Same as above Used on SEM applications especially for light elements in heavy matrix Bence Albee Use in SEM applications especially for mineral samples MBTS Correction assumes that there is no absorption of x rays...

Page 16: ... down Depress the Retract button to retract the X ray detectors Close the spectra display window Shutdown the Windows software MBTSを選択 定量分析に適切な ラインを選択 Select MBTS Choose the elements and lines for quantification ...

Page 17: ...on 100K 200K Using the condenser stigmators right sub panel make the caustic as round as possible and using the 3rd order stigmators left sub panel make the caustic as symmetrical as possible The 3rd order correction will be slight and the controls should be close to the center positions Be sure to use the correct 3rd order stigmators for the selected mode TEM and ANA mode The correctly aligned ca...

Page 18: ... caustic to the center of the phosphor screen Correct both 1st and 3rd order condenser astigmatism Repeat step 3 until caustic does not move with directionality when passing through crossover This correction requires significant beam tilting if the previous operator used the TEM alignment procedure Insert condenser aperture 3rd or 4th and centering by minimizing the tails of intensity surrounding ...

Page 19: ... screws when passing through crossover Remove the any objective aperture and turn off the column pressure gauge filament by pressing the FILAMENT switch 2 Beam alignments in STEM mode Magnification 100K 200K Depress the STEM left main panel Insert the D STEM DET on left side of column Depress the IMAGE SHIFT centering the black circle on CRT monitor using image shift Adjust the FOCUS CONTRAST and ...

Page 20: ...est Notice When the dead time is too high over 30 select smaller condenser aperture or acquire spectrum from thinner region Open the Analyze menu and select Manual Region of Interest Choose the element and lines for element mapping Open the Image Display and select Xray1 Map1 on left cell ...

Page 21: ...21 Select Acquire Point Dwell Acquire and then set parameter up below Set Scanning Speed to 1 Depress Save image as tiff format with respect to each element ...